Composition for conferring wrinkle resistant properties to fabric and method for preparng the same



United States Patent Office 3,440,198 Patented Apr. 22, 1969 3,440,198 COMPOSITION FOR CONFERRING WRINKLE RESISTANT PROPERTIES TO FABRIC AND METHOD FOR PREPARNG THE SAME Edward D. Szubin, West Caldwell, N.J., assignor to The Ironees Company, Philadelphia, Pa., a corporation of Pennsylvania No Drawing. Filed Feb. 15, 1966, Ser. No. 527,528 Int. Cl. C08g 37/30; D06m /58 US. Cl. 260-294 5 Claims ABSTRACT OF THE DISCLOSURE The present invention is directed to a composition for conferring wrinkle resistant properties to a fabric, and more particularly to a method for preparing the same.

In recent years there has been a termendous advance in the technology of so-called permanent press fabrics.

A wide variety of garments have been made of fabrics which have been either post-cured or pre-cured, These garments achieve a durable crease or pleats, which require little or no ironing after laundering and tumble drying.

However, the application of wrinkle resisting finishes to fabrics in the home has not proven satisfactory. Thus, in the home it is not possible to achieve close regulation of concentration and temperature. In addition, problems such as odor, toxicity, and stability on standing are far more serious in terms of a household product than a product used in a factory.

There has been a long felt need for a composition which would enable a housewife to treat yardgoods so as to convert them to a wrinkle resistant fabric, or to convert non-wash and wear garments to a wash and wear garment.

It is essential for a composition that is to be used in the home that it be relatively non-toxic and relatively odorless. The accurate blending of components must be avoided, since the housewife either lacks quantitative measuring apparatus, or is not prone to use such apparatus. Of course, the composition must not significantly damage the yardgoods or fabric. The processing by the housewife must be simple, and such processing must' be capable of being performed with the relatively rudimentary washing, drying, and ironing facilities available to the average housewife.

The composition must be such that it does not affect colors already within the fabric. Furthermore, the composition should not itself be adversely affected, nor should it adversely affect any finish which is already within the fabric or garment being treated by the housewife.

I have studied the basic types of so-called permanent press finishes described in the literature. I find them to be satisfactory for use in the home by the average housewife.

The present invention has as an object the provision of a composition for achieving a wrinkle-resistant fabric, which composition may be used in the home by a nonskilled user.

This invention has as another object the provision of a process for producing a wrinkle-resistant fabric using rudimentary equipment, and without the necessity for extensive training on the part of the user.

Other objects will appear hereinafter.

These objects are achieved by the composition of the present invention which is intended for usage by a housewife, and for application to ya rdgoods or garments (hereinafter referred to as a fabric) which comprises cellulose, such as cotton or linen, using simple equipment and simple procedures.

The composition is stored as two entities, namely the finish component and the catalyst component.

The finish component comprises dimethylol propylene urea, a cationic emulsion of a crystalline polyolefin resin, emulsified silicone oils, and a nonionic surface active agent. The catalyst component consists of zinc nitrate.

Referring to the finish component:

The dimethylol propylene urea, hereinafter referred to as DMPU constitutes the cellulose reactant, namely the resin portion of the finish component which reacts with the cellulose of the fabric to achieve wrinkle-resistant properties, generally called in the art Permanent press. The concentration of DMPU may be varied within the finish component within the range of about 37.5 to 45 weight percent.

The cationic emulsion of the crystalline olefin polymer constitutes an aqueous emulsion of a crystalline polyolefin, which has been chemically modified so that it is emulsifiable with a cationic emulsifying agent. While both crystalline polyethylene and crystalline polypropylene can be used as the crystalline olefin polymer, high density polyethylene is to be preferred. A suitable chemically modified emulsifiable crystalline high density polyethylene is DQWA-0355 described in Union Carbide Corporation New Product Data Bulletin of Nov. 2, 1964. The physical properties of this polymer are as follows:

Specific gravity 0.975 Molecular weight 2500 Ring and ball melting point F. (132 C.) 270 Brookfield viscosity, cps. 140 C. (284 F.) 400-700 Penetration hardness, 5 sec./ 77 F./mm. 10-

grams 0.5 250 grams 0.5-1.0 Acid number 35 Form Flake Color Off white 1 Calculated, not directly measurable.

Another suitable emulsifiable crystalline high density polyethylene is Grex 39 described in Technical Service Bulletin No. of W. R. Grace & Co. The physical properties of this polymer are as follows:

Density, g./cc 0.99 Needle penetration (10ths of a mm.) 05 Acid number 26-28 Viscosity at C., cps 15,000 Ring & ball softening point, C 147 Molecular weight 6500-8500 Armour Ethoxylated Chemicals published by the Amour Industrial Chemical Company.

The acetates are derived by adding between 10 and 20 molar percent excess of acetic acid to the amine.

The cationic emulsion should be present in an amount equivalent to between and weight percent of 27 weight percent aqueous emulsion in which approximately 20 weight percent is the emulsifiable crystalline olefin polymer and 7 weight percent is the cationic emulsifying agent, namely between 1.35 to 2.7 weight percent of the finish component being the non-aqueous portion of the cationic emulsion of the crystalline olefin polymer.

The crystalline olefin polymer confers softening and abrasion resistant properties to the fiinsh component.

The non-ionic silicone oil emulsion constitutes an aqueous emulsion of siloone oils, such as dimethylpolysiloxane having a viscosity at 25 C. of between 200 and 1000 centistokes, emulsified with a suitable emplsifying agent, such as sorbitan monooleate, polyoxyethylene sorbitan monooleate, or an alkyl phenol adduct of ethylene oxide, such as an adduct derived from 6 to mols of ethylene oxide per mol of octylphenol or nonylphenol, or mixtures of these emulsifying agents.

By Way of example of the emulsified silicone oils, the dimethylpolysiloxane silicones having a viscosity at 25 C. of between 200 and 1000 centistokes described in Union Carbide L-45 Silicone Fluid Product Information Bulletin was emulsified with a mixture of sorbitan monooleate and po'lyoxyethylene sorbitan monooleate to produce an aqueous emulsion consisting of 30 percent of the silicone, 2.5 to 3.5 percent of the above mixture of emulsifiers, with the remainder being water. This emulsion may be present in the finish component to the extent of between 0.6 to 1.8 weight percent based on the silicone.

The non-ionic surface active agent effects penetration of the finish component into the cellulose of the fabric. The non-ionic surface active agent should be substantially equivalent to between 0.2 to 0.6 weight percent of nonyl phenol adduct with ethylene oxide derived from between 9 and 10 mols of ethylene oxide per mol of nonyl phenol; a large variety of such agents are known.

The finish component is formed by mixing the aforesaid aqueous mixture of :37.5 to 45 parts by weight of DMPU; 1.35 to 2.7 parts by weight of crystalline olefin polymer emulsified with a cationic emulsifying agent; 0.6 to 1.8 parts by weight of a silicone oil emulsified with a non-ionic emulsifying agent, and 0.2 to 0.6 parts by weight of a non-ionic surface active agent equivalent to amples; an aqueous emulsion of emulsified silicone or 30 weight percent of dimethylpolysiloxane having a viscosity at 25 C. of 500 centistokes and 3 weight percent of a mixture of equal amounts of sorbitan monooleate and polyoxethylene sorbitan monooleate (0.81 Weight percent of the non-aqueous component of the silicone oil) and 8.3 weight percent of the non-ionic surface active agent derived from 9 to 10 mols of ethylene oxide per mol of nonyl phenol was homogenously blended.

This finish component mixture is used by the housewife after being diluted with from 70 to 90 weight percent of water. Preferably a 15 weight percent aqueous homogeneous mixture of the aforesaid finish component and 75 Weight percent added water is preferred for usage by the housewife.

The relative concentrations of the components are not critical, and within the general framework heretofore set forth there is a considerable tolerance for concentration variation.

The finish component of Example 1 diluted to a 15 weight percent aqueous solution was applied to a cotton broadcloth shirt as set forth below with a zinc nitrate catalyst (7 parts by weight diluted finish component to 1 part by weight of 30 weight percent aqueous solution of anhydrous Zinc nitrate). This shirt, after being ironed, had a durable crease which was non-puckered, not broken, and virtually unimpaired after washings. The shirts color was unaffected and there was no noticeable yellowmg.

EXAMPLES 2 THROUGH 9 FINISH COMPONENT In the following examples, the weight percent concentrations, as expressed, are based on a weight percent aqueous solution of dimethylol propylene urea designated DMPU in the examples; a 27 weight percent aqueous cationic emulsion of DQWA-0355 consisting of 20 Weight percent of DQWA-0355 and 7 weight percent of Ethomeen S/15 acetate designated S/15" in the examples; an aqueous emulsion of emulsified silicone or consisting of 30 weight percent of dimethylpolysiloxane having a viscosity at 25 C. of 350 centistokes, and 2.5 to 3.5 weight percent of sorbitan monooleate and polyoxyethylene sorbitan monooleate designated Sil in the examples; and the nonionic surface active agent of the nonyl phenol adduct of ethylene oxide containing between 9 and 10 mols of ethylene oxide per mol of nonyl phenol designated as N in the examples; and with additional water being present in Examples 2, 3, 4,

a nonyl phenol adduct with ethylene oxide derived from 50 6 and 7:

Example 2 3 4 5 6 7 3 9 between 9 and 10 mols of ethylene oxide per mol of nonyl phenol under agitation to achieve a homogeneous mixture. The temperature of blending is not critical and may range from ambient temperatures to below boiling.

The following constitute examples of finish components in accordance with the present invention:

EXAMPLE 1 When each of Examples 2 through 9 is used by the housewife as a finish component, it is diluted with an additional 70 to weight percent of water. A preferred concentration range is about 15 to 20 weight percent. Above about 20 Weight percent there is a noticeable odor, and below about 12 weight percent the finish component is relatively weak.

As above-indicated, catalyst component is zinc nitrate. The catalyst component should be supplied to the housewife as an aqueous solution of zinc nitrate containing between about 14 to 45 weight percent of anhydrous zmc nitrate.

The processing of cellulose fabrics with the finish component and catalyst component of the present invention is as follows:

The user should blend the finish component with the catalyst component prior to usage. The relative ratios of these components in the form used by the housewife, namely after the finish component in the ratios of Examples 1 through 9 has been diluted with an additional 70 to 90 weight percent of water, may vary between 4 to 7 parts by weight of the finish component per part by weight of the catalyst component (concentration of zinc nitrate in catalyst component equal to 30 weigh percent based on anhydrous zinc nitrate). Preferably, the finish component in the form used by the housewife is first blended with from 4 to 8 times its weight of water in a sink, plastic or enameled container (a galvanized bucket should be avoided), after which the catalyst component is added to the dilute mixture. The cellulosic fabric should be soaked within the solution for several minutes. The soaked cellulosic fabric should then be removed, with the excess'dripping being allowed to fall back into the container. Drain drying should be used rather than wring drying so that the fabric is uniformly treated. The fabric should be dried while it is completely flat.

When the fabric is dry to the touch, it is ironed with a dry iron set at the highest possible limit of recommended fabric temperature. No sprinkling is effected during ironing. The ironing should be firmly applied in those regions where creases or pleats are desired.

Any odor or discoloration will disappear after the first washing.

Cross-linking of the resin occurs during drying and during pressing, coupled with a reaction between the resin and the cellulose.

The compositions of the present invention confer excellent wrinkle-resistant and durable crease properties on a cellulosic fabric when processed as above-indicated. The need for elaborate equipment and close control of parameters is avoided. Moreover, any user following simple driections can ac'heive the desiderata. The finish component and catalyst component may be stored indefinitely as such.

I have determined that nine nitrate is the optimum catalyst for use in the subject invention. Thus, I have worked with other catalysts heretofore used in connection with so-called permanent press compositions, such as magnesium chloride, and have found them to be unsatisfactory. In addition, I have determined that for application by the unskilled user, dimethylol propylene urea is far superior to any cellulose reactant tested by me. Thus, I have experimented with urea-glyoxal-formaldehyde reaction products and have found them to be unsatisfactory because they lead to discoloration when used under nonclosely controlled conditions. I have worked with a wide variety of methylol carbamate derivatives, and have found them to be unsatisfactory because of their obnoxious odor, and their poor performance in the absence of closely controlled conditions.

The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof and, accordingly, reference should be made to the appended claims, rather than to the foregoing specification as indicaing the scope of the invention.

It is claimed:

1. A composition for conferring wrinkle resistant properties to a cellulosic fabric, when the composition is blended with a zinc nitrate catalyst, consisting essentially of an aqueous homogeneous mixture in the approximate weight ratio of 37.5 to 45 parts by weight of dimethylol propylene urea, 1.35 to 2.7 parts by weight of crystalline olefin polymer emulsified with a cationic emulsifying agent, 0.6 to 1.8 parts by weight of a silicone oil emulsified with a non-ionic emulsifying agent, and a non-ionic surface active agent in an amount substantially equivalent to 0.2 to 0.6 parts by weight of the nonyl phenol adduct with ethylene oxide derived from between 9 and 10 mols of ethylene oxide per mol of nonyl phenol.

2. A composition in accordance with claim 1 in which the crystalline olefin polymer emulsified with a cationic emulsifying agent is a modified emulsifiable high density,

polyethylene and a cationic emulsifying agent consisting of the acetate salt of a tertiary amine having 1 fatty alkyl group having from 12 to 18 carbon atoms and 2 polyoxyethylene groups attached to the nitrogen.

3. A composition in accordance with claim 1 in which the silicone oil emulsified with a non-ionic emulsifying agent is dimethylpolysiloxane having a viscosity at 25 C. of between 200 and 1000 centistokes.

4. In a composition for conferring wrinkle resistant properties to a cellulosic fabric, a finish component consisting essentially of an aqueous homogeneous mixture in the approximate weight ratio of 37.5 to 45 parts by weight of dimethylol propylene urea, 1.35 to 2.7 parts by weight of crystalline olefin polymer emulsified with a cationic emulsifying agent, 0.6 to 1.8 parts by weight of a silicone oil emulsified with a non-ionic emulsifying agent, and a non-ionic surface active agent in an amount substantially equivalent to 0.2 to 2.6 parts by weight of the nonyl phenol adduct with ethylene oxide derived from between 9 and 10 mols of ethylene oxide per mol of nonyl phenol, and a catalyst component consisting of an adequate amount of zinc nitrate to effect the catalytic reaction between the finish component and the cellulosic fabric required to confer wrinkle resistant properties on the cellulosic fabric.

5. A process for conferring wrinkle resistant properties upon a cellulosic fabric which comprises soaking the cellulosic fabric in a mixture of the composition of claim 4, drain drying the cellulosic fabric and then pressing the cellulosic fabric with a heated iron.

Corp. New York, 1962; 144147.

MURRAY TILLMAN, Primary Examiner. J. T. GOOLKASIAN, Assistant Examiner.

US. Cl. X.R. 8115.6, 116.3; 117-139.4; 260-854 

